CN112850657A - Flue gas separation and purification system for producing electronic-grade sulfuric acid - Google Patents
Flue gas separation and purification system for producing electronic-grade sulfuric acid Download PDFInfo
- Publication number
- CN112850657A CN112850657A CN202110165500.0A CN202110165500A CN112850657A CN 112850657 A CN112850657 A CN 112850657A CN 202110165500 A CN202110165500 A CN 202110165500A CN 112850657 A CN112850657 A CN 112850657A
- Authority
- CN
- China
- Prior art keywords
- tank
- acid
- sulfuric acid
- nicotinic acid
- flue gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/90—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention relates to a flue gas separation and purification system for producing electronic-grade sulfuric acid. The system comprises a dust remover, a washing tower, a demister, a nicotinic acid absorption tower, a nicotinic acid evaporating tank and a condensing tank which are connected in sequence, wherein the washing tower and the nicotinic acid absorption tower are also connected with a circulating tank and a nicotinic acid cooler in sequence, and 98% sulfuric acid solution is arranged at the bottom of the dust remover, at the bottom of the demister and in the circulating tank; the upper portion of the condensing tank body is provided with a water inlet structure, the water inlet structure comprises a first tube plate arranged on the upper portion of the condensing tank body, a cooling water distribution pipe arranged on the inner side of the tank body is connected to the upper portion of the cooling water distribution pipe, a water distribution ring plate is arranged on the inner side of the cooling water distribution pipe, a notch is formed in the upper portion of the water distribution ring plate, the lower portion of the water distribution ring plate is arranged on the first tube plate, a heat exchange tube is vertically arranged in the first tube plate, and the top of the heat exchange tube stretches out of the first tube plate and is evenly. The system can be used for obtaining high-purity sulfur trioxide, and when sulfur trioxide is condensed, no pressure exists in the heat exchange pipe, so that the safety is improved.
Description
Technical Field
The invention relates to the technical field of electronic-grade sulfuric acid production, in particular to a flue gas separation and purification system for producing electronic-grade sulfuric acid.
Background
The electronic grade sulfuric acid is also called high-purity sulfuric acid and ultrapure sulfuric acid, belongs to an ultra-clean high-purity reagent, is a high and new technology product combining electronic materials and fine chemical engineering, is widely applied to cleaning and etching of silicon wafers in the assembling and processing processes of semiconductors and very large scale integrated circuits, and can effectively remove impurity particles, inorganic residues and carbon deposits on the wafers. With the development of large-scale, ultra-large-scale and extremely-large-scale Integrated Circuits (ICs), the chip integration level is higher and higher, the photolithographic lines on the surface of the wafer are thinner and thinner, and the requirements on the quality of electronic-grade sulfuric acid are stricter and stricter.
The preparation process of the electronic-grade sulfuric acid mainly adopts an industrial sulfuric acid rectification method or industrial SO3The liquid is used as raw material to evaporate and absorb.
The industrial sulfuric acid rectification method is a distillation method for separating liquid mixture to high purity by using industrial sulfuric acid through reflux, and comprises normal pressure rectification and reduced pressure rectification. Specifically, the industrial sulfuric acid is firstly pretreated, a strong oxidant (such as potassium permanganate) is added to oxidize reductive impurities in the sulfuric acid into sulfuric acid or carbon dioxide, the treated sulfuric acid is added into a quartz rectifying tower to be rectified, the atmospheric rectifying temperature generally reaches 330 ℃, the reduced pressure rectifying temperature generally reaches 170-190 ℃, the pressure is 1.3-2.5 Kpa, the rectified sulfuric acid is collected into a storage tank, and a microporous filter membrane is used for filtering to remove fine solid impurities to obtain the product.
Industrial SO3The liquid evaporation absorption method adopts industrial SO3The liquid enters an absorption tower through evaporation, and is absorbed by high-purity sulfuric acid.
The rectification method has large energy consumption, small yield and high production cost, and the sulfuric acid produced by the method is difficult to reach the electronic grade sulfuric acid standard which really meets the requirements of integrated circuits due to the problem of equipment used for distilling the sulfuric acid at high temperature.
Industrial SO3Liquid distillation gas absorption method, raw material SO3High cost of liquid due to SO3Liquid is not easy to store and transport, and SO3Difference in purity of liquid, separation of impuritiesThe separation is difficult, so that the quality of the electronic grade sulfuric acid is difficult to improve.
In order to reduce the cost, the method can depend on a non-ferrous smelting acid-making system, non-ferrous smelting flue gas generated by non-ferrous smelting, such as copper smelting flue gas, lead-zinc smelting flue gas, pyrite smelting flue gas and the like, wherein SO is contained in the non-ferrous smelting flue gas3Gas, introduction of SO-containing gas3The sulfur trioxide obtained by separating, purifying, condensing, heating and evaporating the flue gas of the gas is used for preparing electronic-grade sulfuric acid.
The existing nonferrous smelting flue gas mainly adopts a wet purification process, namely the high-temperature nonferrous smelting flue gas is directly reduced to be below 150 ℃ in a water spraying, temperature reducing and quenching mode. In the process, the arsenic trioxide can be desublimated and separated out, and the acid is promoted to condense, so that the sludge mixed with the arsenic trioxide, the waste acid and the dust is finally obtained. But impurities in the flue gas in the technology cannot be radically removed, so that the purity of sulfur trioxide cannot be guaranteed.
Generally, the condensation of sulfur trioxide is carried out in industrial production by using a shell and tube condenser. The shell and tube condenser uses a plurality of heat exchange tubes, cooling water is easy to be unevenly distributed, and the condensation effect of sulfur trioxide is poor. Certain pressure is exerted to the heat exchange pipe to the cooling water, therefore traditional sulfur trioxide condenser has the cracked risk of heat exchange pipe, in case take place the water leakage and advance sour system accident, can reduce the acid fast and concentrated and release a large amount of heats, if discover untimely, can cause serious equipment to damage and environmental pollution accident, so need regularly overhaul or change in order to ensure not to leak water, just so increased the cost of sulfur trioxide condensation in the intangible. The traditional condensing device has low safety and is easy to cause safety accidents. The utility model discloses a chinese utility model patent that publication number is CN 206019383U discloses a vertical novel sulfur trioxide gas condenser, and this condenser is vertical structure, and the lower extreme does not have a pipe case, and during cooling water dropped to an independent water catch bowl to the water catch bowl was disconnected with the condenser, wherein the setting of water catch bowl, when making when the heat exchange tube crack appear, during water was difficult to get into the sulfur trioxide of shell side, and flow away to the water catch bowl internal flow that the resistance is littleer easily.
Disclosure of Invention
The invention provides a flue gas separation and purification system for producing electronic-grade sulfuric acid, aiming at solving the problems that a device for preparing sulfur trioxide by flue gas separation and purification in the prior art cannot remove impurities in flue gas to obtain high-purity sulfur trioxide, cooling water is unevenly distributed when the sulfur trioxide is condensed, and the cooling water applies pressure to a heat exchange pipe, so that the safety is not high. Utilize this system can obtain high-purity sulfur trioxide, when the sulfur trioxide condensation, the cooling water adopts zigzag overflow mode to intake, can make each water inlet of even distribution of cooling water, lets gaseous can the even cooling condensation, does not have pressure in the heat exchanger pipe simultaneously, has improved the security.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a flue gas separation and purification system for producing electronic-grade sulfuric acid comprises a dust remover, a washing tower, a demister, a nicotinic acid absorption tower, a nicotinic acid evaporation tank and a condensation tank which are sequentially connected, wherein the washing tower and the nicotinic acid absorption tower are also sequentially connected with a circulating tank and a nicotinic acid cooler, 98% sulfuric acid solution is respectively arranged at the bottoms of the dust remover and the demister, and 98% sulfuric acid solution is arranged in the circulating tank;
the water inlet structure is arranged on the upper portion of the tank body of the condensing tank and comprises a first tube plate arranged on the upper portion of the tank body of the condensing tank, a cooling water distribution pipe is further arranged on the inner side of the tank body of the condensing tank, the upper portion of the cooling water distribution pipe is connected with a cooling water inlet pipe, a water distribution annular plate is arranged on the inner side of the cooling water distribution pipe, a notch is formed in the upper portion of the water distribution annular plate, the lower portion of the water distribution annular plate is arranged on the first tube plate, a heat exchange tube is vertically arranged in the first tube plate, and a plurality of notches are formed in the top.
According to the preferable scheme, partition plates are arranged above the inner portions of the dust remover and the demister, a plurality of filters are arranged below the partition plates, the tops of the filters penetrate through the partition plates to be fixed, a first mother acid tank is connected below the filters, and analytically pure sulfuric acid is arranged in the first mother acid tank.
Preferably, an acid inlet is arranged below the circulating tank, an acid outlet is arranged at the top of the washing circulating tank, and the acid outlet is connected with a circulating pump.
Preferably, acid separators are arranged at the tops of the washing tower and the nicotinic acid absorption tower, the nicotinic acid cooler provides cooled acidic liquid for the washing tower or the nicotinic acid absorption tower through the acid separators, and a filler layer is arranged below the acid separators.
Preferably, the filters are cylindrical, one filter is positioned in the center of the dust remover or the demister, the other filters are arranged along the circumferential direction of the inner side of the high-temperature dust remover, and the first mother acid tank is cylindrical.
As a preferred scheme, a second mother acid groove is formed in the bottom of a tank body of the nicotinic acid evaporating tank, a first tube plate and a second tube plate are arranged above the second mother acid groove, a plurality of heat exchange tubes are arranged between the first tube plate and the second tube plate of the nicotinic acid evaporating tank, the top of each heat exchange tube of the nicotinic acid evaporating tank penetrates through the first tube plate and then is fixed, a plurality of baffle plates are uniformly arranged between the first tube plate and the second tube plate of the nicotinic acid evaporating tank, the baffle plates are vertically fixed on the side wall of the tank body of the nicotinic acid evaporating tank, a filter is arranged above the first tube plate of the nicotinic acid evaporating tank, and a wire mesh demister is arranged above the.
Preferably, the cooling water distribution pipes are uniformly arranged along the circumferential direction of the tank body of the condensing tank, and a gap is reserved between the cooling water distribution pipes and the first tube plate of the condensing tank.
Preferably, the upper part of the water diversion ring plate is provided with a sawtooth-shaped notch, and the bottoms of the sawtooth-shaped notches are all positioned on the same horizontal plane.
Preferably, the water diversion ring plates are positioned on the peripheries of all heat exchange tubes of the condensing tank, notches in the tops of the heat exchange tubes of the condensing tank are rectangular, and the bottoms of the notches are positioned at the same horizontal height above the first tube plate of the condensing tank.
Preferably, the length of the heat exchange tube of the condensing tank on the first tube plate is less than the height of the water dividing ring plate.
Through the technical scheme, the invention has the beneficial effects that:
1. the invention can remove and absorb impurities and particles in the flue gas through multiple purifications of a dust remover, a demister, a nicotinic acid evaporator and the like; in addition, the temperature of the fuming sulfuric acid is adjusted according to the circulating cooling water in the nicotinic acid cooler, so that the fuming sulfuric acid can fully absorb sulfur trioxide in the flue gas, and the generated waste gas returns to a large system for purification without harming the environment.
2. As a preferable scheme of the invention, the dust remover is provided with a plurality of filters, so that impurity and particulate matters in the flue gas can be better removed. The acid distributor comprises a pipeline and a plurality of spray heads below the pipeline, so that the acid liquid can be uniformly sprayed above the packing layer. The cooling pipeline in the nicotinic acid cooler is of a bent structure, so that the flowing time of the acid liquid in the nicotinic acid cooler is longer, and the acid liquid is more fully cooled.
3. As the preferred scheme of the invention, the nicotinic acid evaporation tank takes the waste high-temperature flue gas as a heat source, the heat source moves upwards along the baffle plate in the tank body, and the nicotinic acid liquid moves upwards in the heat exchange tube, so that the problem that the U-shaped heat exchange tube is required to be used because the heat source moves in the heat exchange tube in the conventional vertical nicotinic acid evaporation device is solved (the U-shaped heat exchange tube has high processing difficulty in production, high manufacturing cost and complicated splicing and installation of the U-shaped heat exchange tube).
4. The cooling water inlet structure of the invention ensures that the cooling water enters the water in an overflow mode, and the heat exchange tube has no pressure, thereby improving the use safety. The arrangement of the gaps formed above the water distribution pipes and the water distribution ring plate can ensure that cooling water is uniformly distributed in each heat exchange pipe to play a role in uniformly cooling and condensing; a plurality of gaps are uniformly formed in the top of the heat exchange tube, so that cooling water can uniformly overflow into the heat exchange tube, and the pressure of the cooling water on the heat exchange tube is greatly reduced.
5. As a preferable scheme of the invention, the sulfur trioxide non-condensable gas exhaust port of the condensing tank can exhaust uncooled sulfur trioxide gas in the tank, so that the excessive pressure in the pipe body is prevented.
6. The plurality of baffle plates are uniformly arranged between the first tube plate and the second tube plate of the nicotinic acid evaporating pot and the condensation pot, so that the heat transfer effect is improved, and the heat exchange tubes can be supported.
Drawings
FIG. 1 is a schematic diagram of a flue gas separation and purification system for producing electronic-grade sulfuric acid according to the present invention.
FIG. 2 is a schematic diagram of a dust collector in a flue gas separation and purification system for producing electronic-grade sulfuric acid.
FIG. 3 is a schematic structural diagram of an isolation plate, a first filter and a first mother acid tank in a flue gas separation and purification system for producing electronic-grade sulfuric acid.
FIG. 4 is a schematic diagram of the structure of a nicotinic acid evaporator in a flue gas separation and purification system for producing electronic-grade sulfuric acid.
FIG. 5 is a schematic diagram of the first tube plate, heat exchange tube and baffle plate of the nicotinic acid evaporator in the flue gas separation and purification system for producing electronic-grade sulfuric acid.
FIG. 6 is a schematic diagram of the baffle plate of the nicotinic acid evaporator in the flue gas separation and purification system for producing electronic-grade sulfuric acid.
FIG. 7 is a schematic diagram of the condenser in the flue gas separation and purification system for producing electronic-grade sulfuric acid according to the present invention.
FIG. 8 is a first structural diagram of the water inlet structure of the condenser in the flue gas separation and purification system for producing electronic-grade sulfuric acid.
FIG. 9 is a schematic structural diagram II of a water inlet structure of a condenser in a flue gas separation and purification system for producing electronic-grade sulfuric acid.
FIG. 10 is a schematic structural diagram of a heat exchange tube of a condenser in a flue gas separation and purification system for producing electronic-grade sulfuric acid.
The reference numbers in the drawings are as follows: 1 is a dust remover, 12 is a separation plate, 14 is a first filter, 15 is a first mother acid tank, 2 is a washing tower, 22 is an acid distributor, 23 is a packing layer, 3 is a circulating tank, 32 is a circulating pump, 4 is a demister, 5 is a nicotinic acid absorption tower, 6 is a nicotinic acid evaporating tank, 61 is a second mother acid tank, 62 is a second filter, 63 is a wire mesh demister, 64 is a flue gas outlet, 65 is a flue gas inlet, 66 overflow ports, 67 is a viewing mirror, 7 is a condensing tank, 71 is a cooling water distribution pipe, 72 is a cooling water inlet pipe, 73 is a water distribution ring plate, 74 is a non-condensable gas exhaust port, 8 is a nicotinic acid cooler, 101 is a first tube plate, 102 is a second tube plate, 103 is a heat exchange pipe, and 104 is a baffle plate.
Detailed Description
The invention is further described with reference to the following figures and detailed description:
as shown in fig. 1 to 10, the flue gas separation and purification system for producing electronic-grade sulfuric acid of the present embodiment includes a dust remover 1, a washing tower 2, a demister 4, a nicotinic acid absorption tower 5, a nicotinic acid evaporation tank 6 and a condensation tank 7, which are connected in sequence, and the washing tower 2 and the nicotinic acid absorption tower 5 are also connected in sequence with a circulation tank 3 and a nicotinic acid cooler 8.
Specifically, the gas outlet of the dust remover 1 is connected with the gas inlet of the washing tower 2 through a pipeline, the gas outlet of the washing tower 2 is connected with the gas inlet of the high-efficiency demister 4 through a pipeline, the gas outlet of the demister 4 is connected with the gas inlet of the nicotinic acid absorption tower 5 through a pipeline, the acid outlet of the washing tower 2 is connected with the acid inlet of the washing circulation tank 3 through a pipeline, the acid outlet of the washing circulation tank 3 is connected with a circulating pump 32, the circulating pump 32 pumps acid liquor for the nicotinic acid cooler 8, and the nicotinic acid cooler 8 supplies the cooled acid liquor to the washing tower 2 through the acid distributor 22. The acid outlet of nicotinic acid absorption tower 5 passes through the pipe connection with absorption circulation tank 3's acid inlet, absorption circulation tank 3's acid outlet is connected with circulating pump 32, circulating pump 32 is to nicotinic acid cooler 8 or 6 pump sending acidizing fluids of nicotinic acid evaporating pot, wherein nicotinic acid cooler 8 provides the acidizing fluid after the cooling to nicotinic acid absorption tower 5 through dividing acid ware 22, circulating pump 32 passes through the nicotinic acid entry of second mother acid groove 61 on the pipe connection nicotinic acid evaporating pot 6, the sulfur trioxide gas export of nicotinic acid evaporating pot 6 passes through the sulfur trioxide gas entry of pipe connection condensing pot 7.
An isolation plate 12 is arranged above the interior of the dust remover 1, a plurality of first filters 14 are arranged below the isolation plate 12, the tops of the first filters 14 penetrate through the isolation plate 12 for fixing, and a first mother acid groove 15 is connected below the first filters 14; the first filters 14 are cylindrical, one first filter 14 is positioned in the center of the high-temperature dust remover 1, and the other first filters 14 are circumferentially arranged along the inner side of the high-temperature dust remover 1; due to the action of the isolation plate 12, the flue gas can only enter the top of the high-temperature dust remover 1 through the filter 14, and the filter element of the first filter 14 is a PET (polyethylene terephthalate) filter element, so that impurities in the flue gas can be well filtered and attached to the surface of the first filter 14; the first mother acid tank 15 is cylindrical, analytically pure sulfuric acid is arranged in the first mother acid tank, the upper part of the first mother acid tank is connected with the first filter 14 through a pipeline, when high-temperature flue gas enters the dust remover 1, the analytically pure sulfuric acid volatilizes and adheres to the surface of the first filter 14 to form acid dew, impurities on the surface of the first filter 14 are dissolved, and the service life of the first filter 14 is prolonged; the bottom of the dust remover 1 is provided with 98 percent refined sulfuric acid solution, impurities falling off after acid dew is dissolved can be removed and absorbed, and the 98 percent sulfuric acid solution needs to be replaced periodically, so that the cleanness and the purity of sulfur trioxide are ensured.
The top of the washing tower 2 is provided with an acid distributor 22, a packing layer 23 is arranged below the acid distributor 22, the acid distributor 22 comprises a pipeline and a plurality of spray heads below the pipeline, the spray heads are uniformly distributed on the pipeline, acid liquor from the washing circulation tank 3 can be uniformly sprayed on the packing layer 23 through the acid distributor 22, the packing of the packing layer 23 in the washing tower 2 is quartz ceramic packing, so that the acid liquor on the packing layer 23 and flue gas passing through an air inlet can be sufficiently combined, and impurities and particles in the flue gas can be removed and absorbed.
An acid inlet is formed in the lower left of the washing circulating tank 3, an acid outlet is formed in the top of the washing circulating tank 3, the acid outlet is connected with a circulating pump 32, and 98% refined sulfuric acid solution is arranged in the washing circulating tank 3.
The inside top of defroster 4 is provided with division board 12, the below of division board 12 is provided with a plurality of first filters 14, division board 12 is passed at the top of first filter 14 and is fixed, the below of first filter 14 is connected with first mother acid groove 15, and first mother acid groove 15 is inside to be provided with the analytically pure sulphuric acid, first filter 14 is cylindrically, and one of them first filter 14 is located high-efficient defroster 4's central authorities, other first filters 14 arrange along high-efficient defroster 4 inboard circumference. The bottom of the demister 4 is also provided with 98% refined sulfuric acid solution, which can remove and absorb impurities falling off after the acid dew is dissolved.
The top of the nicotinic acid absorption tower 5 is provided with an acid distributor 22, a packing layer 23 is arranged below the acid distributor 22, and the packing of the packing layer 23 in the nicotinic acid absorption tower 5 is tetrafluoro packing.
An acid inlet is formed in the lower left of the absorption circulation tank 3, an acid outlet is formed in the top of the absorption circulation tank 3, the acid outlet is connected with a circulation pump 32, and 98% refined sulfuric acid solution is arranged in the absorption circulation tank 3.
The inside cooling tube that is provided with of nicotinic acid cooler 8, cooling tube is the structure of buckling, and its both ends connect the acid inlet and the acid outlet of nicotinic acid cooler 8 respectively. The nicotinic acid cooler 8 supplies the cooled acid solution to the washing column 2 or the nicotinic acid absorption column 5 through the acid distributor 22.
The tank body of the nicotinic acid evaporating tank 6 is of a vertical cylindrical structure made of stainless steel; a second mother acid tank 61 is arranged at the bottom of the nicotinic acid evaporator 6, nicotinic acid liquid can be contained in the second mother acid tank 61, a circulating pump 32 is arranged in the second mother acid tank 61, a first tube plate 101 and a second tube plate 102 are arranged above the circulating pump 32, the side edges of the first tube plate 101 and the second tube plate 102 of the nicotinic acid evaporator 6 are attached to the side wall of the tank body and then fixed, a plurality of heat exchange tubes 103 are arranged between the first tube plate 101 and the second tube plate 102 of the nicotinic acid evaporator 6, the top of each heat exchange tube 103 of the nicotinic acid evaporator 6 passes through the first tube plate 101 and then is fixed, the bottom of each heat exchange tube 103 passes through the second tube plate 102 and then is connected with the circulating pump 32 through a pipeline, and the circulating pump 32 can pump the nicotinic acid liquid in the second mother acid tank 61 to the upper part of the first tube; a flue gas inlet 65 is arranged close to the first tube plate 101, and a flue gas outlet 64 is arranged close to the second tube plate 102; a plurality of baffle plates 104 are uniformly arranged between the first tube plate 101 and the second tube plate 102, the baffle plates 104 are in a single arch shape and are vertically fixed on the side wall of the tank body, two adjacent baffle plates 104 are oppositely arranged, a plurality of circular holes are distributed on the surface of each baffle plate 104, and a heat exchange tube 103 passes through each circular hole; the above-mentionedAn overflow port 66 and a sight glass 67 are arranged above the first tube plate 101, the overflow port 66 and the sight glass 67 are flush, the inside of the tank body can be seen through the sight glass 67, the circulating pump 32 pumps the nicotinic acid liquid to the upper part of the first tube plate 101, and when the nicotinic acid liquid reaches the position of the sight glass 67, the nicotinic acid liquid flows into the second mother acid tank 61 from the overflow port 66 through a pipeline, so that the nicotinic acid liquid above the first tube plate 101 is always kept at the position flush with the sight glass 67; the second filter 62 is arranged above the overflow port 66, the wire mesh demister 63 is arranged above the second filter 62, the second filter 62 and the wire mesh demister 63 are both cylindrical, the side edges of the second filter 62 and the wire mesh demister 63 are attached to the side wall of the tank body, and the evaporated SO can be treated3The gas is purified and demisted again, further ensuring SO3The purity of the gas; and a sulfur trioxide gas outlet is formed in the upper part of the metal wire mesh demister 63 and is positioned at the top of the tank body 6 of the nicotinic acid evaporating tank.
The jar body of condensing jar 7 is vertical structure, and the jar body upper portion of condensing jar 7 is provided with the cooling water structure of intaking, and is concrete, and the jar body 7 upper portion of condensing jar is provided with first tube sheet 101, and the internal side of jar of condensing jar 7 is provided with cooling water distributing pipe 71, cooling water inlet tube 72 is connected on cooling water distributing pipe 71 upper portion, and cooling water distributing pipe 71 is provided with 6 and evenly sets up along 7 jar body circumference of condensing jar for the cooling water that gets into from cooling water inlet tube 72 evenly intakes to condensing jar 7 from 6 directions.
A gap is left between the cooling water distribution pipe 71 and the first tube plate 101 so that the cooling water can flow out from the cooling water distribution pipe 71.
The inner side of the cooling water distribution pipe 71 is provided with a water distribution ring plate 73, the upper part of the water distribution ring plate 73 is provided with a zigzag notch, the bottom of the zigzag notch is positioned on the same horizontal plane, the lower part of the water distribution ring plate 73 is arranged on a first pipe plate 101, a heat exchange pipe 103 is vertically arranged in the first pipe plate 101, the top of the heat exchange pipe 103 extends out of the first pipe plate 101 and is uniformly provided with a plurality of rectangular notches, and the bottoms of the rectangular notches are positioned at the same horizontal height above the first pipe plate 101. The bottom of the water dividing ring plate 73 is welded and sealed with the first tube plate 101, and the water dividing ring plate 73 is positioned on the periphery of all the heat exchange tubes 103. The structure enables the cooling water flowing out of the cooling water distributing pipe 71 to overflow into each heat exchange pipe 103, and solves the problems that the water inlet distribution is uneven and the heat exchange pipe 103 is easy to crack due to the pressure formed on the heat exchange pipe 103 when the cooling water directly enters the water in the prior art.
The length of the heat exchange tube 103 on the first tube sheet 101 is less than the height of the water dividing ring plate 73.
The bottom cooling water outlet of the tank body of the condensing tank 7, the second tube plate 102 is arranged above the cooling water outlet, the heat exchange tube 103 is positioned between the first tube plate 101 and the second tube plate 102, the top of the heat exchange tube 103 penetrates through the first tube plate 101 and the bottom of the heat exchange tube 102 penetrates through the second tube plate 102, the upper end of the tank body between the first tube plate 101 and the second tube plate 102 is provided with a sulfur trioxide gas inlet and a sulfur trioxide noncondensable gas exhaust port 74, and the lower end of the tank body is provided with a sulfur trioxide condensate outlet.
The tank body of the condensing tank 7 is of a cylindrical structure made of stainless steel, and a support is arranged on the periphery of the tank body of the condensing tank 7 to facilitate the fixation of the tank body. And a sulfur trioxide non-condensable gas exhaust port 74 is formed in the side wall opposite to the sulfur trioxide gas inlet on the tank body of the condensing tank 7, so that excessive sulfur trioxide non-condensable gas in the tank body of the condensing tank 7 is prevented from causing excessive gas pressure in the tank.
A plurality of baffle plates 104 are uniformly arranged between the first tube plate 101 and the second tube plate 102 of the condensation tank 7, the baffle plates 104 are made of stainless steel materials, the baffle plates 104 are vertically fixed on the side wall of the tank body of the condensation tank 7, the baffle plates 104 are in a single arc shape, two adjacent baffle plates 104 are oppositely arranged, a plurality of circular holes are distributed on the surfaces of the baffle plates 104, a heat exchange tube 103 penetrates through each circular hole, the baffle plates 104 enable sulfur trioxide gas to flow in the tank body in a turning-back manner, so that the condensation of sulfur trioxide is more sufficient, and meanwhile, the baffle plates 104 can be used for supporting the.
When the device is used, flue gas enters from the air inlet of the dust remover 1 and enters the upper part of the dust remover 1 through the PET polyester fiber filter, the flue gas after primary filtration enters the washing tower 2 through the air outlet of the dust remover 1 through a pipeline, then the filler layer 23 in the washing tower 2 is combined with 98% refined sulfuric acid solution to remove and absorb impurities in the flue gas, the dust removal efficiency of the dust remover 1 is more than or equal to 98%, the outlet dust mist quantity diameter of the dust remover 1 is less than 1 mu m, and the temperature is less than or equal to 190 ℃. The 98% refined sulfuric acid solution is firstly pumped out by a circulating pump 32, then is cooled by a nicotinic acid cooler 8, and finally is sprayed by an acid separator 22 to flow downwards to a packing layer 23, the flue gas filtered by the 98% refined sulfuric acid solution enters a demister 4 from a gas outlet of a washing tower 2, the temperature of the flue gas entering the high-efficiency demister 4 is less than or equal to 110 ℃, the flue gas is filtered again by a fiber filter in the demister 4, the efficiency of the demister 4 is more than or equal to 98%, then the flue gas enters a nicotinic acid absorption tower 5 through a pipeline, the flue gas entering the nicotinic acid absorption tower 5 is fully purified, then the 98% refined sulfuric acid in an absorption circulating tank 3 is pumped to the acid separator 22 by the circulating pump 32 to be sprayed, the sulfur trioxide gas in the nicotinic acid absorption tower 5 is absorbed and concentrated to form fuming sulfuric acid (commonly called as nicotinic acid), and the gas after being separated returns to a large-.
The oleum is pumped into the second mother acid tank 61 of the nicotinic acid evaporator 6 by the circulating pump 32. Then, the waste high-temperature flue gas enters the tank body of the nicotinic acid evaporation tank 6 from the flue gas inlet 65 of the nicotinic acid evaporation tank 6, the flue gas moves along the baffle plate 104, at this time, the nicotinic acid liquid in the second mother acid tank 61 at the bottom of the tank body of the nicotinic acid evaporation tank 6 is pumped to the upper part of the first tube plate 101 through the circulating pump 32, and when the nicotinic acid liquid moves upwards through the heat exchange tube 103, the high-temperature flue gas heats the nicotinic acid liquid in the heat exchange tube 103, SO that SO is evaporated from the nicotinic acid liquid3Gas, post SO3The gas continues to move upwards through a second filter 62 and a wire demister 63 for purification and demisting, and finally SO3The gas is discharged through a sulfur trioxide gas outlet and then enters the condensation tank 7 through a sulfur trioxide gas inlet of the condensation tank 7.
During condensation, the cooling water inlet pipe 72 is communicated with an external cooling water supply pipeline, the cooling water outlet is communicated with a water cooling tower, cooling water enters the tank body of the condensation tank 7 from the cooling water inlet pipe 72, specifically, the cooling water is uniformly distributed on the periphery of the water distribution ring plate 73 through the water distribution pipe 71, the cooling water overflows to the inner side of the water distribution ring plate 73 from the zigzag notches on the water distribution ring plate 73, then the cooling water uniformly flows into the heat exchange pipe 103 from the rectangular groove at the top of the heat exchange pipe 103, and finally the cooling water is recovered through the cooling water outlet. The sulfur trioxide gas flows in the tank body of the condensation tank 7 along the baffle plate 104, the cooling water in the heat exchange pipe 103 condenses the sulfur trioxide gas, and the sulfur trioxide condensate flows downward through the baffle plate 104 and then is discharged through the sulfur trioxide condensate outlet. Cooling water in this condensation jar 7 adopts the overflow mode to intake, divides the water through the zigzag breach of dividing the water ring board 73, can make cooling water evenly distributed to heat exchange tube 103, guarantees sulfur trioxide gas's condensation effect, does not have pressure in the heat exchange tube 103 simultaneously, improves the security.
The above-described embodiments are merely preferred embodiments of the present invention, and not intended to limit the scope of the invention, so that equivalent changes or modifications in the structure, features and principles described in the present invention should be included in the claims of the present invention.
Claims (10)
1. The flue gas separation and purification system for producing electronic-grade sulfuric acid is characterized by comprising a dust remover (1), a washing tower (2), a demister (4), a nicotinic acid absorption tower (5), a nicotinic acid evaporation tank (6) and a condensation tank (7) which are sequentially connected, wherein the washing tower (2) and the nicotinic acid absorption tower (5) are also sequentially connected with a circulating tank (3) and a nicotinic acid cooler (8), 98% sulfuric acid solution is respectively arranged at the bottoms of the dust remover (1) and the demister (4), and 98% sulfuric acid solution is arranged in the circulating tank;
the upper portion of the tank body of the condensation tank (7) is provided with a water inlet structure, the water inlet structure comprises a first tube plate (101) arranged on the upper portion of the tank body of the condensation tank (7), the inner side of the tank body of the condensation tank (7) is further provided with a cooling water distribution pipe (71), the upper portion of the cooling water distribution pipe (71) is connected with a cooling water inlet pipe (72), the inner side of the cooling water distribution pipe (71) is provided with a water distribution annular plate (73), the upper portion of the water distribution annular plate (73) is provided with a notch, the lower portion of the water distribution annular plate is arranged on the first tube plate (101), a heat exchange tube (103) is vertically arranged in the first tube plate (101), and the top of the heat exchange tube (103) stretches out of the.
2. The flue gas separation and purification system for producing electronic-grade sulfuric acid according to claim 1, wherein a partition plate (12) is arranged above the inner part of each of the dust collector (1) and the demister (4), a plurality of first filters (14) are arranged below the partition plate (12), the tops of the first filters (14) penetrate through the partition plate (12) for fixing, a first mother acid tank (15) is connected below the first filters (14), and analytically pure sulfuric acid is arranged in the first mother acid tank (15).
3. The flue gas separation and purification system for producing electronic-grade sulfuric acid according to claim 1, wherein an acid inlet is arranged below the circulation tank (3), an acid outlet is arranged at the top of the washing circulation tank (3), and the acid outlet is connected with a circulation pump (32).
4. The flue gas separation and purification system for producing electronic-grade sulfuric acid according to claim 1, wherein an acid separator (22) is arranged at the top of each of the washing tower (2) and the nicotinic acid absorption tower (5), the nicotinic acid cooler (8) supplies cooled acid liquid to the washing tower (2) or the nicotinic acid absorption tower (5) through the acid separator (22), and a packing layer (23) is arranged below the acid separator (22).
5. A flue gas separation and purification system for the production of electronic grade sulfuric acid according to claim 2, characterized in that the first filters (14) are cylindrical, one of the first filters (14) is located in the center of the dust collector (1) or the demister (4), the other first filters (14) are arranged circumferentially along the inside of the dust collector (1), and the first mother acid tank (15) is cylindrical.
6. The flue gas separation and purification system for producing electronic-grade sulfuric acid according to claim 1, wherein a second mother acid tank (61) is arranged at the bottom of the nicotinic acid evaporation tank (6), a first tube plate (101) and a second tube plate (102) are arranged above the second mother acid tank (61), a plurality of heat exchange tubes (103) are arranged between the first tube plate (101) and the second tube plate (102) of the nicotinic acid evaporation tank (6), the top of the heat exchange tubes (103) of the nicotinic acid evaporation tank (6) passes through the first tube plate (101) and then is fixed, a plurality of baffle plates (104) are uniformly arranged between the first tube plate (101) and the second tube plate (102) of the nicotinic acid evaporation tank (6), the baffle plates (104) are vertically fixed on the side wall of the nicotinic acid evaporation tank (6), and a second filter (62) is arranged above the first tube plate (101) of the nicotinic acid evaporation tank (6), a wire mesh demister (63) is arranged above the second filter (62).
7. The flue gas separation and purification system for producing electronic-grade sulfuric acid according to claim 1, wherein the cooling water distribution pipe (71) is provided in plurality and uniformly arranged along the circumferential direction of the condensation tank (7), and a gap is left between the cooling water distribution pipe (71) and the first tube plate (101) of the condensation tank (7).
8. The flue gas separation and purification system for producing electronic-grade sulfuric acid according to claim 1, wherein the upper part of the water diversion ring plate (73) is provided with a zigzag notch, and the bottoms of the zigzag notch are all in the same horizontal plane.
9. The flue gas separation and purification system for producing electronic-grade sulfuric acid according to claim 1, wherein the water diversion ring plate (73) is located at the periphery of all heat exchange tubes (103) of the condensation tank (7), the gap at the top of the heat exchange tubes (103) of the condensation tank (7) is rectangular, and the bottom of the gap is located at the same horizontal height above the first tube plate (101) of the condensation tank (7).
10. The flue gas separation and purification system for the production of electronic grade sulfuric acid according to claim 1, characterized in that the heat exchange tubes (103) of the condensing tank (7) are located on the first tube plate (101) with a length less than the height of the water dividing ring plate (73).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110165500.0A CN112850657B (en) | 2021-02-06 | 2021-02-06 | Flue gas separation and purification system for producing electronic-grade sulfuric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110165500.0A CN112850657B (en) | 2021-02-06 | 2021-02-06 | Flue gas separation and purification system for producing electronic-grade sulfuric acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112850657A true CN112850657A (en) | 2021-05-28 |
| CN112850657B CN112850657B (en) | 2022-11-25 |
Family
ID=75988734
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110165500.0A Active CN112850657B (en) | 2021-02-06 | 2021-02-06 | Flue gas separation and purification system for producing electronic-grade sulfuric acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112850657B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113546437A (en) * | 2021-08-10 | 2021-10-26 | 联仕(昆山)化学材料有限公司 | Electronic-grade sulfuric acid production system and production process |
| CN115535971A (en) * | 2021-06-29 | 2022-12-30 | 杭州瑞佑科技有限公司 | Method for preparing high-purity electronic grade sulfuric acid from waste sulfuric acid solution |
Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4307069A (en) * | 1976-05-20 | 1981-12-22 | David Lurie | Desulfurization of flue gases with complete sulfite oxidation |
| US5695616A (en) * | 1995-09-27 | 1997-12-09 | Virginia Accelerators Corporation | Electron beam flue gas scrubbing treatment |
| CN1537499A (en) * | 2003-04-17 | 2004-10-20 | 潘忠勋 | Healt-charging insulation shower device |
| JP2008232485A (en) * | 2007-03-19 | 2008-10-02 | Matsushita Electric Ind Co Ltd | Ventilating air conditioner |
| US20100139579A1 (en) * | 2006-09-15 | 2010-06-10 | Shaohua Su | Water heater special for bathroom |
| CN101936673A (en) * | 2009-06-30 | 2011-01-05 | 江苏中兴化工设备有限公司 | Macroporous plate convergent-divergent pipe efficient heat exchanger |
| CN101954198A (en) * | 2010-09-03 | 2011-01-26 | 镇江正丹化学工业有限公司(外商独资) | High-pressure dehydrating tower in process of continuously producing trimellitate |
| CN102424369A (en) * | 2011-10-17 | 2012-04-25 | 上海奥格利环保工程有限公司 | Production process for reagent grade high-purity sulfuric acid |
| CN203518100U (en) * | 2013-09-29 | 2014-04-02 | 西安工程大学 | Vertical tube type indirect evaporative cooling air conditioner |
| CN203899437U (en) * | 2014-05-15 | 2014-10-29 | 淮南市明月环保科技有限责任公司 | Tower tank fume gas purification system |
| CN105947994A (en) * | 2016-04-29 | 2016-09-21 | 上海京藤化工有限公司 | Production device and production method for MOS-grade sulfuric acid used for microelectronics |
| CN106430117A (en) * | 2016-10-21 | 2017-02-22 | 河池市生富冶炼有限责任公司 | Method for preparing analytical pure sulfuric acid by using smelting flue gas |
| CN106482113A (en) * | 2016-12-12 | 2017-03-08 | 北京神雾环境能源科技集团股份有限公司 | A kind of heat accumulating type deflection plate electronic gas refuse pyrolysis system |
| CN107445379A (en) * | 2017-08-25 | 2017-12-08 | 金川集团股份有限公司 | A kind of device and method of acid waste water evaporation emission reduction |
| CN207861893U (en) * | 2017-12-22 | 2018-09-14 | 上海乐谦工程科技有限公司 | One kind is novel to pass through SO3The system that absorption process prepares AR grades of sulfuric acid |
| CN111908432A (en) * | 2020-09-09 | 2020-11-10 | 江苏庆峰工程集团有限公司 | Production method and production device for refining 98% sulfuric acid for electronic industry |
-
2021
- 2021-02-06 CN CN202110165500.0A patent/CN112850657B/en active Active
Patent Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4307069A (en) * | 1976-05-20 | 1981-12-22 | David Lurie | Desulfurization of flue gases with complete sulfite oxidation |
| US5695616A (en) * | 1995-09-27 | 1997-12-09 | Virginia Accelerators Corporation | Electron beam flue gas scrubbing treatment |
| CN1537499A (en) * | 2003-04-17 | 2004-10-20 | 潘忠勋 | Healt-charging insulation shower device |
| US20100139579A1 (en) * | 2006-09-15 | 2010-06-10 | Shaohua Su | Water heater special for bathroom |
| JP2008232485A (en) * | 2007-03-19 | 2008-10-02 | Matsushita Electric Ind Co Ltd | Ventilating air conditioner |
| CN101936673A (en) * | 2009-06-30 | 2011-01-05 | 江苏中兴化工设备有限公司 | Macroporous plate convergent-divergent pipe efficient heat exchanger |
| CN101954198A (en) * | 2010-09-03 | 2011-01-26 | 镇江正丹化学工业有限公司(外商独资) | High-pressure dehydrating tower in process of continuously producing trimellitate |
| CN102424369A (en) * | 2011-10-17 | 2012-04-25 | 上海奥格利环保工程有限公司 | Production process for reagent grade high-purity sulfuric acid |
| CN203518100U (en) * | 2013-09-29 | 2014-04-02 | 西安工程大学 | Vertical tube type indirect evaporative cooling air conditioner |
| CN203899437U (en) * | 2014-05-15 | 2014-10-29 | 淮南市明月环保科技有限责任公司 | Tower tank fume gas purification system |
| CN105947994A (en) * | 2016-04-29 | 2016-09-21 | 上海京藤化工有限公司 | Production device and production method for MOS-grade sulfuric acid used for microelectronics |
| CN106430117A (en) * | 2016-10-21 | 2017-02-22 | 河池市生富冶炼有限责任公司 | Method for preparing analytical pure sulfuric acid by using smelting flue gas |
| CN106482113A (en) * | 2016-12-12 | 2017-03-08 | 北京神雾环境能源科技集团股份有限公司 | A kind of heat accumulating type deflection plate electronic gas refuse pyrolysis system |
| CN107445379A (en) * | 2017-08-25 | 2017-12-08 | 金川集团股份有限公司 | A kind of device and method of acid waste water evaporation emission reduction |
| CN207861893U (en) * | 2017-12-22 | 2018-09-14 | 上海乐谦工程科技有限公司 | One kind is novel to pass through SO3The system that absorption process prepares AR grades of sulfuric acid |
| CN111908432A (en) * | 2020-09-09 | 2020-11-10 | 江苏庆峰工程集团有限公司 | Production method and production device for refining 98% sulfuric acid for electronic industry |
Non-Patent Citations (1)
| Title |
|---|
| 潘先桐等: "冷凝器与冷却水", 《发酵科技通讯》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115535971A (en) * | 2021-06-29 | 2022-12-30 | 杭州瑞佑科技有限公司 | Method for preparing high-purity electronic grade sulfuric acid from waste sulfuric acid solution |
| CN115535971B (en) * | 2021-06-29 | 2024-02-09 | 杭州瑞佑科技有限公司 | Method for preparing high-purity electronic grade sulfuric acid from waste sulfuric acid solution |
| CN113546437A (en) * | 2021-08-10 | 2021-10-26 | 联仕(昆山)化学材料有限公司 | Electronic-grade sulfuric acid production system and production process |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112850657B (en) | 2022-11-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112850657B (en) | Flue gas separation and purification system for producing electronic-grade sulfuric acid | |
| CN102161541B (en) | Method for extracting salt from coking desulphurization waste solution and special device thereof | |
| CN107362568B (en) | The method of high efficiente callback solvent in a kind of production of high-performance carbon fibre | |
| CN106831526A (en) | Reclaim, purify the device and method of N methyl pyrrolidones | |
| CN113651693A (en) | Equipment and method for producing ethyl acetate by using ionic liquid dehydration technology | |
| CN206467171U (en) | Reclaim, purify the device of N methyl pyrrolidones | |
| CN112897474B (en) | Device for purifying sulfur trioxide | |
| CN205461092U (en) | Rectification system | |
| CN209161961U (en) | A kind of purification-recovery system for damaged tire cracking oil gas | |
| CN111578303A (en) | Purification system and method for recycling flue gas waste heat in stepped mode | |
| CN101874985B (en) | Film evaporation concentrating method and device | |
| CN215609419U (en) | N-methyl diisopropanolamine continuous rectification device | |
| CN201245444Y (en) | Quartz glass fractionating tower | |
| RU2517524C2 (en) | Method and apparatus for processing hydrogen in purification unit of terephthalic acid purification device | |
| CN208599441U (en) | A kind of equipment of NMP recycling purification | |
| CN214528147U (en) | Sulfur trioxide purifying device | |
| CN113603112A (en) | Device for preparing electronic-grade ammonia water and preparation process thereof | |
| CN217449521U (en) | Spray recovery tower | |
| CN205527750U (en) | Sulphuric acid purification device | |
| CN217264858U (en) | AR-grade sulfuric acid preparation system with three-stage purification | |
| CN215026044U (en) | Nicotinic acid evaporation plant | |
| CN103771370B (en) | The device of electron-level phosphoric acid is produced in a kind of U-tube crystallization | |
| CN216946214U (en) | Purification cleaning system for anhydrous hydrogen fluoride reaction gas | |
| CN219922094U (en) | Useless ethanol dewatering purification device | |
| CN218478542U (en) | Wet-process acid making system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |